Effect of Steeping Corn with Lactic Acid on Starch Properties

Pasting and thermal properties of starch from corn steeped in the presence of lactic acid and at different steeping times (8, 16, 24, 32, and 40 hr) were investigated. Corn kernels were steeped at 52°C with 0.2% (w/v) SO₂ and with and without 0.5% (v/v) lactic acid. The isolated starch obtained by corn wet‐milling was characterized by determining starch recoveries, retrogradation, and melting transition properties of the lipid‐amylose complex by differential scanning calorimetry (DSC), and pasting properties by the Rapid Visco Analyser (RVA). Damaged granules and the starch granule size were determined by using microscopic techniques. Starches from corn steeped in the presence of lactic acid (LAS) were compared with control starch (CS) steeped without lactic acid. Greater starch recoveries were obtained for LAS samples than for CS samples, and practically no damaged starch was present in the former preparations. The presence of lactic acid affected the RVA profiles and steeping time affected the viscosities of the starch suspensions. In general, the RVA parameters of LAS suspensions were lower than those of CS suspensions. No great modification of the thermal properties was observed; only a slight decrease in amylopectin retrogradation and in the melting enthalpy of the amylose‐lipid complex was observed. Hydrolysis of the starch during steeping seems the most probable explanation to the starch modifications produced by lactic acid addition.     

Effect of Steeping with Sulfite Salts and Adjunct Acids on Corn Wet‐Milling Yields and Starch Properties

Two corn hybrids (3394 and 33R87) were steeped with three sulfite salts and five acids to test the effect of sulfur dioxide (SO₂) source and acid sources on wet‐milling yields and starch properties. Milling yields from each treatment were compared with a control sample that was steeped with 2,000 ppm of SO₂ (using sodium metabisulfite) and 0.55% lactic acid. Sulfur dioxide sources were potassium sulfite, sodium sulfite, and ammonium sulfite; acids were acetic, hydrochloric, oxalic, phosphoric, and sulfuric. Starch yields were affected by the SO₂ source and steep acids but the effects were hybrid‐dependent. Different steep acids gave different starch yields when wet milled at the same pH. Among the acids tested, weak acids (lactic and acetic) tended to give higher starch yields compared with strong acids (hydrochloric, sulfuric, phosphoric, and oxalic). Some differences were observed with different sulfite salts and acids on starch pasting properties; however, there were no clear trends.     

Batch Steeping of Corn: Effects of Adding Lactic Acid and Sulfur Dioxide at Different Times on Starch Yields,Protein Contents,and Starch Pasting Properties

The effect of adding lactic acid and sulfur dioxide at different times from the start of batch steeping on corn starch yields was studied. Five commercial hybrids were steeped with 0.5% lactic acid or 0.2% sulfur dioxide added over the first 15 hr of steeping and wet-milled following a 100-g corn wet-milling procedure. No significant differences were observed in starch yields when lactic acid was added to the steep solution (SO₂ and water) from 0 hr (start of steeping) to 15 hr. Addition of SO₂ to the steep solution (lactic acid and water) resulted in significantly higher average starch yields when SO₂ was added between 5 and 15 hr compared with addition at 0 hr (SO₂ and lactic acid for full 24 hr of steeping). Based on the results of the first experiment, a second experiment was done in which one of five original hybrids was steeped for 24 hr, during which lactic acid or SO₂ was added until 23.9 hr (i.e., 5 min before milling) after the start of steeping. Similar results were found in the second experiment. Residual protein in starch samples did not exceed 0.85%. Steepwater protein content decreased with delays (16–20 hr) in adding either chemical to the steep solution. A significant effect on starch pasting properties of chemicals and duration of chemicals in steep-water was observed. Testing these findings using a larger scale (1,000 g) corn wet-milling procedure produced results similar to those obtained with the 100-g corn wet-milling procedure.     

Hybrid-Dependent Effect of Lactic Acid on Corn Starch Yields

The effect of lactic acid on starch yields of different corn hybrids was determined by wet-milling 18 commercial corn hybrids at three levels of lactic acid. All 18 hybrid samples tested had higher starch yields when lactic acid was added to the steep solution, although the magnitude of the increased starch yields varied between 2.9 and 12.0%. The optimal lactic acid concentration for maximum starch recovery was found to be between 0.55 and 1.67% lactic acid, by wet-milling nine of the same 18 corn hybrids with seven levels of added lactic acid. Between 0.83 and 1.67% lactic acid, the starch yields of eight of the nine hybrids were constant (within ±0.5%). Results showed that the average starch yield across all hybrids decreased with a lactic acid concentration <0.55% and a lactic acid concentration >1.67%.     

Effect of Steeping Conditions (Sulfur Dioxide,Lactic Acid,and Temperature) on Starch Yield,Starch Quality,and Germ Quality from the Intermittent Milling and Dynamic Steeping Process (IMDS) for a Brazilian Corn Hybrid

Effect of lactic acid, SO₂, temperature, and their interactions were assessed on the dynamic steeping of a Brazilian dent corn (hybrid XL 606) to determine the ideal relationship among these variables to improve the wet‐milling process for starch and corn by‐products production. A 2×2×3 factorial experimental design was used with SO₂ levels of 0.05 and 0.1% (w/v), lactic acid levels of 0 and 0.5% (v/v), and temperatures of 52, 60, and 68°C. Starch yield was used as deciding factor to choose the best treatment. Lactic acid added in the steep solution improved the starch yield by an average of 5.6 percentage points. SO₂ was more available to break down the structural protein network at 0.1% than at the 0.05% level. Starch‐gluten separation was difficult at 68°C. The lactic acid and SO₂ concentrations and steeping temperatures for better starch recovery were 0.5, 0.1, and 52°C, respectively. The Intermittent Milling and Dynamic Steeping (IMDS) process produced, on average, 1.4% more starch than the conventional 36‐ hr steeping process. Protein in starch, oil content in germ, and germ damage were used as quality factors. Total steep time can be reduced from 36 hr for conventional wet‐milling to 8 hr for the IMDS process.     

Effect of Chemical Pretreatments and Lactic Acid on the Rate of Water Absorption and Starch Yield in Corn Wet-Milling

The relative effectiveness of dehulling, potassium hydroxide dipping (alkali concentrations 0.2, 0.5, and 1.0 %), and ethyl oleate spraying (aqueous emulsion 1%, v/v) to increase the rate of water absorption by dent and flint corn during steeping was compared with untreated corn samples. These pretreatments increased the water absorption rate of both hybrids when compared with the untreated control samples. To evaluate the observed increase, the diffusion coefficients of pretreated and untreated corn samples were estimated. Corn grains steeped in SO₂ aqueous solution and variable lactic acid concentrations (0.2, 0.5, and 1.0%, v/v) were performed. Absorption rates for lactic acid concentrations were ≈0.5% higher than those steeped only in SO₂ solution. This effect was more marked for dent than for flint corn. Corn samples pretreated with potassium hydroxide had lower starch yields than the control. However, the presence of lactic acid in steepwater increased the starch yield of dent and flint corn, particularly for the samples treated with alkaline solution. This procedure was particularly beneficial for flint corn. An effective release of the starch granules was achieved within 24 hr of steeping.     

Effect of Laboratory Batch Steeping pH on Starch Yield and Pasting Properties of Selected Corn Hybrids

This study evaluated the effect of initial pH on percent of starch yield and pasting characteristics for a laboratory wet‐milling procedure. Four commercial hybrids, selected because they have significantly different starch yield values, were laboratory wet‐milled, and the pasting properties of the starch fractions were evaluated using a Rapid Visco Analyser (RVA). Percent starch yield (db) decreased when initial pH values were >4.0 but was unaffected by any lower initial pH values. The pasting properties of some of the selected hybrids were more sensitive to steepwater pH than others. There was an overall increase in peak, trough, and final viscosity as pH increased.     

Yield,Protein Content,and Viscosity of Starch from Wet‐Milled Corn Hybrids as Influenced by Environmentally Induced Changes in Test Weight

Forty‐three yellow dent corn samples of five different hybrids varying in test weight and moisture content were obtained from 14 different locations in 1993. The locations for acquired samples were selected randomly to cover a wide range of test weights based on preliminary data from eight states of the corn belt where 94% of the U.S. corn crop was produced in 1993. Samples were wet‐milled using a 100‐g standard laboratory‐scale wet‐milling procedure. Protein content in starch and starch viscosity were determined. Starch yield, protein content in starch, and starch viscosity were not affected significantly by test weight.     

Effect of Stress Cracks on Corn Wet‐Milling Yields

U.S. No. 2 yellow dent corn was randomly probe‐sampled from rail cars being shipped to a wet‐milling plant from a Corn Belt local elevator. The probe samples were blended together and kernels were sorted into four levels of stress cracks (0, 1, 2, or multiple). Each level of stress cracking was then laboratory wet‐milled in triplicate. The only statistically observed differences were in total fiber and in protein content of the gluten meal fraction. The starch yield difference between zero stress cracked corn and multiple stress cracked corn was smaller (0.8%) than would be expected if stress cracking were an indicator of damage to the wet‐milling characteristics of the corn.     

Effects of Selected Harvest Moistures and Frozen Storage Times on Selected Yellow Dent Corn: Wet‐Milling Yields and Starch Pasting Properties

The effects of harvest moistures and frozen storage times on corn wet‐milling yields and the pasting properties of the resulting starch were studied. Pioneer hybrid P‐0916‐XR harvested at three moisture contents (49, 35, and 21% wb) were stored frozen for three days or for five months, followed by wet‐milling. The pasting properties of the resulting starch were evaluated with a Rapid Visco Analyzer. The yields of starch and germ increased by 1.2 and 1.9 percentage points, respectively, when harvest moisture decreased from 49 to 21% wb, whereas the yields of steep water solids, total fiber, and gluten decreased by 2.1, 0.7, and 0.6 percentage points, respectively. The frozen corn had lower coarse fiber yields but higher cellular fiber yields. The starch pasting properties showed that peak and breakdown viscosities decreased by 8% (3,824 ± 36 versus 3,520 ± 38 cP) and 13% (2,336 ± 47 versus 2,029 ± 60 cP), respectively, when harvest moisture decreased from 49 to 21% wb, whereas peak time increased by 5% (6.32 ± 0.06 versus 6.62 ± 0.07 min). The setback and final viscosities of starch from long‐term frozen storage (five months) were 14% (1,574 ± 65 versus 1,828 ± 79 cP) and 8% (3,063 ± 27 versus 3,317 ± 101 cP) lower, respectively, than that from control (unfrozen) corn.     

Pasting Properties and Surface Characteristics of Starch Obtained from an Enzymatic Corn Wet‐Milling Process

Recently, we reported the development of an enzymatic corn wet‐milling process that reduces or eliminates sulfur dioxide requirements during steeping, considerably reduces steep time, and produces starch yields comparable to that of conventional corn wet‐milling. The best results so far, using the enzymatic corn wet‐milling procedure, were achieved when a particular protease enzyme (bromelain) was used. In this study, pasting properties and surface characteristics of starch obtained from six different enzyme treatments (three glycosidases [β‐glucanase, cellulase, and xylanase] and three proteases [pepsin, acid protease, and bromelain]) using the enzymatic corn wet‐milling procedure were evaluated and compared with those from starch obtained using the conventional corn wet‐milling procedure. Significant effects from enzymatic milling were observed on all the three starch pasting properties (peak, shear thinning, and setback). The setback viscosities of starch from all enzyme treatments were significantly lower compared with those of the control sample, indicating that starch polymers from enzymatic corn wet‐milling do not reassociate to the same extent as with the control. Comparison between bromelain treatment and the control sample showed that starch samples obtained from bromelain treatment are very similar to control starch in water‐binding capacity, molecular breakdown, and time to swell when cooked in water. Significant effects from enzymatic milling were observed on the surface characteristics of starch granules. The glycosidase treatments, especially the β‐glucanase samples, showed holes in the starch granules. No visual differences were observed in starch granules between bromelain and control samples.     

Effects of Maturity on Grain Quality and Wet‐Milling Properties of Two Selected Corn Hybrids

The effects of maturity on grain quality and wet‐milling properties were investigated for two hybrids of corn. Significant differences for hybrid and maturity were observed for all grain quality parameters. Test weight, absolute density, and thousand‐grain weight all increased as the corn matured. Kernel hardness increased and breakage susceptibility varied with increased maturity. Water uptake parameters decreased with maturity of the grain. The starch yield results from wet milling showed that the starch yield increased significantly within each cultivar in the early stages of grain maturity, but there were no significant differences between hybrids. Mathematical models using selected grain quality parameters accurately predicted trends in starch yield for the immature and mature corn samples in this study.     

Wet‐Milling and Dry‐Milling Properties of Dent Corn with Addition of Amylase Corn

A transgenic corn (amylase corn) has been developed that produces an endogenous α‐amylase that is activated in the presence of water and elevated temperature (>70°C). Wet‐ and dry‐milling characteristics of amylase corn were evaluated using laboratory wet‐ and dry‐milling procedures. Different amounts of amylase corn (0.1–10%) were added to dent corn (with the same genetic background as the amylase corn) as treatments. Samples were evaluated for wet‐ and dry‐milling fraction yields using 1‐kg laboratory procedures. Milling yields for all amylase corn treatments were compared with the control treatment (0% amylase corn or 100% dent corn). No significant differences were observed in wet‐ and dry‐milling yields between the control and the 0.1, 1, and 10% amylase corn treatments. Most of the amylase activity (77%) in wet‐milling fractions was detected in the protein fraction. In dry‐milling, amylase activity (68.8%) was detected in endosperm fractions (fines, small grits, and large grits).     

Effects of Alkali Debranning,Roller Mill Cracking and Gap Setting,and Alkali Steeping Conditions on Milling Yields from a Dent Corn Hybrid

Starch yield was significantly affected by all three main unit operations in alkali wet‐milling (debranning, roller milling, and steeping). The conditions for the three unit operations were studied using a single hybrid. Studies on debranning showed that optimal separation between pericarp and corn endosperm was obtained when corn was soaked in a 1.5–2% NaOH solution at 85°C for 5 min. Passing debranned corn through smooth roller mill once or twice did not affect the product yields, but passing the corn through the roller mill three times decreased the germ yield because of a large amount of broken germ. A 62% higher processing rate could be achieved when passing corn through the mill twice than by passing it through the mill once. The gap should be set at 2.0 mm when passing corn through the mill once, and it should be set at 3.5 mm for the first pass and 2.0 mm for the second pass when passing corn through the mill twice. Starch yield was more sensitive to NaOH concentration and steep temperature than to steep time. The highest starch yield was obtained when steeping corn in 0.5% NaOH for 1 hr at 45°C.     

Effect of a Cell‐Wall‐Degrading Enzyme Complex on Starch Recovery and Steeping Requirements of Sorghum and Maize

The effect of a commercial cell‐wall‐degrading enzyme (CWDE) complex on the steeping time and starch yields of white regular sorghum (RSOR) compared with yellow maize (YMZ) was determined. An in vitro wet‐milling method standardized to test dosages of 0–120 fungal β‐glucanase units (FBG)/100 mL indicated that starch yields were significantly higher for YMZ than RSOR and increased proportionally as enzyme dosage increased. A factorial experiment with a level of confidence of P < 0.05 was performed to study the effect of CWDE addition to coarsely ground grains for 4 hr after 20 or 44 hr of SO₂ steeping of whole grains. At both regular steep times, YMZ yielded significantly higher amounts of starch than RSOR. When steep times were compared, grains soaked for 48 hr produced 1.7% higher starch yields than counterparts treated for 24 hr. CWDE significantly increased starch yields and recoveries. Enzyme‐treated grains yielded 2.5% more starch than counterparts steeped regularly. For both grains, the best wet‐milling conditions to obtain the highest amount of starch were 48 hr of steeping and CWDE addition. Under these conditions, YMZ and RSOR yielded 66.9 and 66.6% starch, respectively. Starches obtained after the enzyme treatment at both steep times contained higher amounts of residual protein and ash compared with the untreated counterparts. Rapid viscoamylograph properties of YMZ and RSOR starches were not affected by the use of the CWDE nor the steep time. In comparison with RSOR starch, the YMZ starch initiated gelatinization at lower temperature, had less shear thinning and higher viscosity or setback at the end of cooling.     

Effect of Mill Plate Setting and Number of Dynamic Steeping Stages for an Intermittent Milling and Dynamic Steeping (IMDS) Process for Corn

Effect of corn degermination mill parameters (clearance between mill plates and rpm) were assessed on the broken germ and number of whole kernels in mash so as to optimize the cracking procedure for the intermittent milling and dynamic steeping (IMDS) process. The dynamic steep time and number of intermittent milling stages for the IMDS process were also optimized for maximum starch recovery. A comparison was made between the IMDS and the conventional steeping process for fraction yields. A clearance of 0.45–0.48 cm between the plates gave the most optimum processing conditions (minimum broken germ and least amount of whole kernels in mash after cracking). Effect of rpm on germ damage and kernel cracking was not significant when optimum clearance between the degermination plates was maintained. Two stages of intermittent milling with a dynamic steep time of 30 min or higher was recommended because it produced the highest yield of starch and germ. Comparison of the IMDS process with the conventional wet‐milling process showed that starch and gluten yield increased by 1.6 and 4.26%, respectively, in the IMDS process. Germ recovered from the IMDS process was 0.54% lower than that from the conventional steeping process.     

Pretreatment of Wet‐Milled Corn Fiber to Improve Recovery of Corn Fiber Oil and Phytosterols

The phytosterol‐containing oil in the corn fiber (corn fiber oil) has potential use as a natural low‐density lipoprotein (LDL) lowering nutraceutical but its low concentration (1–3%) makes it difficult and expensive to extract. Pretreatment of corn fiber with dilute acid or glucosidases removed nonlipid components of fiber, producing oil‐enriched fractions that should be more amenable to efficient and inexpensive oil extraction. Acid, as well as enzymes, significantly increased the content of corn fiber oil and its phytosterol compounds by hydrolyzing (and removing) the starch and nonstarch (cell wall) polysaccharides from the wet‐milled corn fiber. Dual treatment of the fiber with acid and enzyme greatly increased the concentrations of corn fiber oil and its phytosterol components, compared with acid or enzyme treatments alone. Depending on the treatment, the oil concentration in the residual solids increased from 0.3 to 10.8% (21–771% increase in conc.) and the total phytosterol concentration increased from 19.8 to 1256.2 mg/g of fiber (11–710% increase in conc.) compared with untreated fiber.     

Effects of Resistant Starch and Fiber from High‐Amylose Non‐Floury Corn on Tortilla Texture

A high‐amylose, non‐floury corn, a floury corn, and a 1:1 blend were made into masa and then tortillas. The masa flour made with the high‐amylose corn had a greater amount of resistant starch (RS 28.8%) and a greater amount of total dietary fiber (TDF 42.1%) than that with the floury corn (RS 2.9%, TDF 9.6%), producing a high‐fiber tortilla. The masa was evaluated for pasting properties using a Rapid ViscoAnalyser (RVA). The high‐amylose masa slurry gelatinized little at 95°C. The floury masa had the greatest peak viscosity, whereas the 1:1 blend was intermediate in value. Sensory evaluations of the tortillas for the textural attributes showed the floury tortillas to be chewier, more rollable, and grittier than the high‐amylose tortillas, whereas the blend tortillas were intermediate for most attributes. The cutting force of the high‐amylose tortillas, measured on a texture analyzer, was very low; the blend and floury tortillas required more force. Chewiness was correlated to rollability (r = 0.99, P = 0.05). The %RS and %TDF were correlated to rollability (r = –0.99), and cutting force (r = 0.99). The floury and blend tortillas had firm textures expected of desirable tortillas, whereas the high‐amylose tortillas broke under little force, and would not roll. The high‐amylose tortillas had high amounts of RS and TDF but poor texture. The blend tortillas retained most floury tortilla textural properties, making them suitable products for consumer use.     

Comparison of Enzymatic (E‐Mill) and Conventional Dry‐Grind Corn Processes Using a Granular Starch Hydrolyzing Enzyme

A new low temperature liquefaction and saccharification enzyme STARGEN 001 (Genencor International, Palo Alto, CA) with high granular starch hydrolyzing activity was used in enzymatic dry‐grind corn process to improve recovery of germ and pericarp fiber before fermentation. Enzymatic dry‐grind corn process was compared with conventional dry‐grind corn process using STARGEN 001 with same process parameters of dry solid content, pH, temperature, enzyme and yeast usage, and time. Sugar, ethanol, glycerol and organic acid profiles, fermentation rate, ethanol and coproducts yields were investigated. Final ethanol concentration of enzymatic dry‐grind corn process was 15.5 ± 0.2% (v/v), which was 9.2% higher than conventional process. Fermentation rate was also higher for enzymatic dry‐grind corn process. Ethanol yields of enzymatic and conventional dry‐grind corn processes were 0.395 ± 0.006 and 0.417 ± 0.002 L/kg (2.65 ± 0.04 and 2.80 ± 0.01 gal/bu), respectively. Three additional coproducts, germ 8.0 ± 0.4% (db), pericarp fiber 7.7 ± 0.4% (db), and endosperm fiber 5.2 ± 0.6% (db) were produced in addition to DDGS with enzymatic dry‐grind corn process. DDGS generated from enzymatic dry‐grind corn process was 66% less than conventional process.